CN110823749B - Multifunctional high-pressure reaction evaluation device and method - Google Patents
Multifunctional high-pressure reaction evaluation device and method Download PDFInfo
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- CN110823749B CN110823749B CN201911173518.4A CN201911173518A CN110823749B CN 110823749 B CN110823749 B CN 110823749B CN 201911173518 A CN201911173518 A CN 201911173518A CN 110823749 B CN110823749 B CN 110823749B
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Abstract
The invention relates to a multifunctional high-pressure reaction evaluation device and method. The device comprises a high-pressure precision balance system, a reaction furnace system, a gas circuit control system, an oil gas cooling and recovering system and gas online sampling. The high-pressure precision balance system can move up and down along with the lifting system, and a high-pressure sealing ring and an annular coupling piece are arranged at the joint of the high-pressure precision balance system and the reaction furnace system, so that strict sealing under high pressure is realized; the gas circuit control system is connected with the reaction furnace system in a hard sealing mode; the oil gas cooling and recovering system is connected with an oil gas outlet pipeline on the upper part of the reaction furnace system by a clamping sleeve, and cooled gas enters an online chromatograph for online analysis. The invention can realize the reaction processes of pyrolysis, gasification, catalyst evaluation and the like under the harsh conditions of temperature, pressure, atmosphere, heating rate and the like in a high-pressure environment, and has the advantages of wide raw material applicability, high precision, wide operation conditions, convenient use, high automation degree and the like.
Description
Technical Field
The invention relates to a high-pressure reaction evaluation device and method, in particular to a multifunctional high-pressure reaction evaluation device and method.
Background
The thermal analysis method is a main method and means for analyzing and testing chemical reactions and physical change processes of solid and liquid reactants, and is widely applied to the fields of energy, chemical engineering, metallurgy, materials, environment and the like. In order to make the thermal analysis conditions closer to reality, the trend of thermal analysis technology is represented by the increase in pressure, temperature, and temperature of the analysis conditions.
The reaction process under the pressurization environment is very complex, the chemical reaction and the transfer processes of mass transfer, heat transfer and the like are influenced by the change of pressure fluctuation, and the basic data such as the transfer rule, the empirical formula, the mathematical model and the like involved in the reaction process are difficult to obtain accurately. The test research under the pressurization condition has more severe requirements on the aspects of design work and test operation such as process flow, instrument precision, equipment material and the like, in order to ensure the smooth operation of the test work, the optimization of the process conditions in the early stage is necessary to be carried out through a pressurization reaction device, the main parameters in the experimental process are artificially controlled, the redundant exploration of the rule of the amplified pressurization test device is reduced, and the reaction rule suitable for the pressurization environment is explored.
At present, the market pressurized thermal analysis technology is in a continuous perfect stage, and the commercialized pressurized thermal analysis technology in foreign countries has high price and poor operability, and is difficult to meet the operation under special atmosphere conditions of water vapor, hydrogen, carbon monoxide and the like. Therefore, the development of a thermal analysis evaluation device which is suitable for the conditions of high pressure and high temperature, water vapor and the like has important scientific significance for improving the research depth of a plurality of fields such as pyrolysis, gasification, catalytic processes and the like.
Disclosure of Invention
The invention aims to provide a multifunctional high-pressure reaction evaluation device and a multifunctional high-pressure reaction evaluation method which have high automation degree and convenient operation and can be used for the research of multiple fields such as pyrolysis, gasification experiments, catalyst evaluation experiments, activity measurement and the like.
In order to achieve the purpose, the evaluation device comprises a high-pressure precision balance system, a reaction furnace system, an oil-gas cooling and recovering system and a gas online sampling and gas path control system:
the high-pressure precision balance system comprises a protective shell (2) which is fixedly arranged on one side of the lifting system and is provided with a protective gas inlet, a high-pressure hanging arm type precision balance is sealed in the protective shell, the lower end of the high-pressure hanging arm type precision balance is connected with one end of a sample lifting hook, and the other end of the sample lifting hook is connected with a sample loader;
the reaction furnace system comprises a high-pressure furnace body with a furnace gas inlet and a furnace gas outlet, and an electric heating element and a high-pressure reaction tube which are arranged in the high-pressure furnace body, wherein two ends of the high-pressure reaction tube extend out of the high-pressure furnace body, the upper end of the high-pressure reaction tube is coupled with a high-pressure precision balance system, a sample lifting hook and a sample loader are vertically arranged in the high-pressure reaction tube, a heat tracing device connected with an oil-gas cooling and recycling system is arranged on the wall of the high-pressure reaction tube extending out of the upper end of the high-pressure furnace body, a reaction gas inlet and a multi-element thermocouple interface are arranged on the wall of the high-pressure reaction tube extending out of the lower end of the high-pressure furnace body from top to bottom, and a temperature measuring element is arranged in the high-pressure reaction tube and connected with the multi-element thermocouple interface;
the oil gas cooling and recovering system comprises a primary cooling section, a secondary cooling section, a high-pressure filter element, a high-pressure precise control valve and a ball valve which are sequentially connected in the flowing direction, wherein a pressurized gas inlet is arranged between the high-pressure precise control valve and the high-pressure filter element, an online gas chromatography detector is also connected between the high-pressure precise control valve and the ball valve, and the primary cooling section is connected with a heat tracing device;
the gas path control system comprises a gas source pressure regulating valve, a gas flow controller, a high-pressure gas hedging mixer and a high-pressure gas preheater which are sequentially connected in the flowing direction, wherein the high-pressure gas preheater is communicated with a reaction gas inlet, one path of a gas source is used as reaction gas to enter the high-pressure gas hedging mixer through the gas source pressure regulating valve and the gas flow controller, the reaction gas enters the high-pressure gas hedging mixer through the high-pressure gas preheater, and the other three paths of the gas source are respectively connected with a protective gas inlet, a furnace gas inlet and a charging gas inlet.
The high-pressure precision balance system is connected with the inner coupling surface of the high-pressure reaction tube in a mode of combining a high-pressure sealing ring and an annular coupling piece.
The precision of the high-pressure hanging arm type precision balance is 1 mu g, the sample loading amount of the high-pressure hanging arm type precision balance and a sample loader is 2-10 g, the highest reaction temperature of the high-pressure reaction tube is 1300 ℃, the reaction pressure is 0.001-7.0 MPa, and the heating rate is 10-150 ℃/min.
The heat tracing device adopts one or more combinations of electric heat tracing, steam heat tracing or oil bath heat tracing.
The first-stage cooling section is a natural convection cooling section, the second-stage cooling section is a forced convection cooling section, the two sections of pipelines are connected by high-pressure detachable clamping sleeves, and cooled gas passes through a high-pressure filter element and then is subjected to gas online sampling for online gas chromatography analysis.
The temperature from the outlet of the high-pressure reaction tube to the primary cooling section is 350-500 ℃, one or more combinations of oleophylic adsorptive quartz cotton, porous carbon materials and oleophylic fiber materials are filled in the primary cooling section, the temperature of the secondary cooling section is-20-0 ℃, a solvent method is adopted to wash and collect a cooling oil sample, namely one or more combinations of volatile solvents of dichloromethane, petroleum ether, acetone and diesel oil are adopted to wash a pipeline of the secondary cooling section, and the cooling oil sample is collected.
The high-pressure filter element is one or a combination of a metal sintering device and a ceramic filter screen, the particle size of the trapped particles is less than 200 mu m, and the high-pressure precise control valve is a pneumatic regulating valve.
The gas source adopts one or more combinations of reaction gases of nitrogen, hydrogen, carbon dioxide, carbon monoxide, air, methane and water vapor, and the reactions comprise thermal cracking reaction, catalytic reaction, pyrolysis reaction, gasification reaction, CO2And (4) performing active reaction.
The high-pressure gas counter-flushing mixer is a multi-channel counter-flushing mixer, the temperature of the reaction gas preheated by the high-pressure gas preheater is more than or equal to 300 ℃, and the inlet of the high-pressure gas counter-flushing mixer is also connected with an electric heating steam generator with a micro plunger pump.
The multifunctional high-pressure reaction evaluation method comprises the following steps:
1) sample loading: placing the weighed sample in a sample loader, and closing a high-pressure precision balance system and a reaction furnace system through a lifting system;
2) heating for reaction: opening an air source, and adjusting an air source pressure adjusting valve to enable the air source pressure to be higher than the experimental pressure by 0.5-1.0 MPa; setting the gas flow of the reaction gas, the protective gas, the furnace gas and the pressurizing gas, setting the pressurizing gas flow to be zero after the system pressure is reached, and controlling the experiment pressure through a high-pressure regulating valve; starting a high-pressure gas preheater, a reactor outlet heat tracing device and an electric heating element, starting reaction when the temperature meets the experimental requirements, and recording and analyzing weightlessness data of a high-pressure balance and data of each temperature and pressure measuring point; simultaneously introducing gas generated by reaction into an online gas chromatography detector through a connecting pipeline for separation and analysis;
3) cooling the reactor: after the experiment is finished, setting the flow of the reaction gas to be zero, closing the high-pressure gas preheater, the reactor outlet heat tracing element and the electric heating element, reducing the pressure to normal pressure through a high-pressure regulating valve according to the pressure relief rate required by the experiment, cooling, and setting the flow of the protective gas and the flow of the furnace gas to be zero when the temperature is reduced to 50-200 ℃; and (4) taking down the annular coupling ring, lifting the high-pressure precision balance system to take down the sample loader, collecting residual substances in the sample loader, and weighing and recording.
The reaction of the invention comprises thermal cracking reaction, catalytic reaction, pyrolysis reaction, gasification reaction and CO2Reactive reactions, and the like but not limited to these reactions. The invention realizes quick pressurization to reach the set pressure under the condition of not influencing the weight change of materials in the device. After the test is finished, the oil-gas-containing pipeline is purged in a mode of switching between steam and heating inert gas, so that product residue is avoided.
Drawings
FIG. 1 is a schematic structural diagram of a multifunctional high-pressure reaction evaluating device.
FIG. 2-1 results of coal pyrolysis under different pressure conditions (N)2Atmosphere);
FIG. 2-2 pyrolysis results of coal at different ramp rates (N)2Atmosphere);
FIGS. 2-3 the pyrolysis results (4.0MPa) of coal under different reaction atmospheres;
FIGS. 2-4 pyrolysis results (N) of different feedstocks (coal, biomass) under the same conditions2Atmosphere);
2-5 total ion current chromatograms of coal pyrolysis oil products under different pressure conditions;
FIG. 3 results of coal pressure gasification reaction (4.0MPa, 30 ℃/min)
FIG. 4 shows the results of the pressurized pyrolysis of coal with catalyst (4.0MPa, 10 ℃/min).
As shown in figure 1, 1-precision balance, 2-protective shell, 3-protective gas inlet, 4-lifting system, 5-high pressure furnace body, 6-electric heating element, 7-high pressure reaction tube, 8-sample hook, 9-sample loader, 10-furnace gas inlet, 11-furnace gas outlet, 12-reaction gas inlet, 13-multi-element thermocouple interface, 14-high pressure gas preheater, 15-high pressure gas counter-flushing mixer, 16-gas flow controller, 17-gas source pressure regulating valve, 18-electric heating steam generator, 19-micro plunger pump, 20-annular coupling piece, 21-high pressure sealing ring, 22-heat tracing device, 23-primary cooling section, 24-secondary cooling section, 25-high pressure filter element, 26-high pressure precision control valve, 27-ball valve, 28-online gas chromatography, 29-charging gas inlet
Detailed Description
The present invention is further illustrated by the following examples, which are provided for illustration only and are not intended to limit the scope of the present invention.
Example 1:
referring to fig. 1, the multifunctional high-pressure reaction evaluation device of the present embodiment includes a high-pressure precision balance system, a reaction furnace system, an oil-gas cooling and recovery system, and a gas online sampling and gas path control system;
the high-pressure precision balance system comprises a protective shell 2 which is fixedly arranged on one side of a lifting system 4 and is provided with a protective gas inlet 3, a high-pressure hanging arm type precision balance 1 is sealed in the protective shell 2, the lower end of the high-pressure hanging arm type precision balance 1 is connected with one end of a sample lifting hook 8, and the other end of the sample lifting hook 8 is connected with a sample loader 9; wherein the precision of the high-pressure hanging arm type precision balance 1 is 1 mu g, and the sample loading amount of the sample loader 9 is 2-10 g;
the reaction furnace system comprises a high-pressure furnace body 5 with a furnace gas inlet 10 and a furnace gas outlet 11, and an electric heating element 6 and a high-pressure reaction tube 7 which are arranged in the high-pressure furnace body 5, wherein two ends of the high-pressure reaction tube 7 extend out of the high-pressure furnace body 5, a high-pressure precision balance system is connected with the inner coupling surface of the high-pressure reaction tube in a way of combining with an annular coupling piece 22 through a high-pressure sealing ring 21, a sample lifting hook 8 and a sample loader 9 are vertically arranged in the high-pressure reaction tube 7, a heat tracing device 22 which is connected with an oil gas cooling and recovering system and adopts one or a plurality of combinations of electric heat tracing, steam heat tracing or oil bath heat tracing is arranged on the tube wall of the high-pressure reaction tube 7 extending out of the lower end of the high-pressure furnace body 5, a reaction gas inlet 12 and a multielement thermocouple interface 13 are arranged from top to bottom, a temperature measuring element is arranged in the tube wall of the high-pressure reaction tube 7 and is connected with the multielement thermocouple interface 13, the highest reaction temperature of the high-pressure reaction tube 7 is 1300 ℃, the reaction pressure is 0.001-7.0 MPa, and the heating rate is 10-150 ℃/min;
the oil gas cooling recovery system comprises a primary cooling section 23, a secondary cooling section 24, a high-pressure filter element 25, a high-pressure precise control valve 26 and a ball valve 27 which are sequentially connected in the flowing direction, wherein a pressurized gas inlet 29 is arranged between the high-pressure precise control valve 26 and the high-pressure filter element 25, an online gas chromatography detector 28 is also connected between the high-pressure precise control valve 26 and the ball valve 27, and the primary cooling section 23 is connected with a heat tracing device 22; the high-pressure filter element 25 is one or a combination of a metal sintering device and a ceramic filter screen, the particle size of the trapped particles is less than 200 mu m, and the high-pressure precision control valve 26 is a pneumatic regulating valve;
the first-stage cooling section 23 is a natural convection cooling section, the second-stage cooling section 24 is a forced convection cooling section, the two sections of pipelines are connected by high-pressure detachable clamping sleeves, and cooled gas passes through a high-pressure filter element 25 and then is subjected to gas online sampling for online gas chromatography analysis;
the temperature from the outlet of the high-pressure reaction tube 7 to the primary cooling section 23 is 350-500 ℃, one or more combinations of oleophylic adsorptive material quartz cotton, porous carbon material and oleophylic fiber material are filled in the primary cooling section 23, the temperature of the secondary cooling section 24 is-20-0 ℃, a solvent method is adopted to wash and collect a cooling oil sample, namely one or more combinations of volatile solvents of dichloromethane, petroleum ether, acetone and diesel oil are adopted to wash a pipeline of the secondary cooling section 24, the cooling oil sample is collected,
the gas path control system comprises a gas source pressure regulating valve 17, a gas flow controller 16, a high-pressure gas hedging mixer 15 and a high-pressure gas preheater 14 which are sequentially connected in the flowing direction, wherein the high-pressure gas preheater 14 is communicated with a reaction gas inlet 12, a gas source is used as reaction gas to enter the high-pressure gas hedging mixer 15 through one path of the gas source pressure regulating valve 17 and the gas flow controller 16 and then enters the reaction gas from the reaction gas inlet 12 through the high-pressure gas preheater 14, the other three paths of the gas source pressure regulating valve 17 and the gas flow controller 16 are respectively connected with a protective gas inlet 3, a furnace gas inlet 10 and a charging gas inlet 29, the high-pressure gas hedging mixer 15 is a multi-pore channel hedging mixer, the temperature of the reaction gas preheated by the high-pressure gas preheater 14 is not less than 300 ℃, and the inlet of the high-pressure gas hedging mixer 15 is also connected with an electric heating steam generator 18 with a micro-plunger pump 19.
The reaction gas adopted by the invention is one or a plurality of combinations of nitrogen, hydrogen, carbon dioxide, carbon monoxide, air, methane and water vapor, and the reaction comprises thermal cracking reaction, catalytic reaction, pyrolysis reaction, gasification reaction, CO2And (4) performing active reaction.
The using method comprises the following steps:
switching on a power supply, lifting the high-pressure precision balance system to a certain height, putting a certain amount of raw materials into the sample loader, closing the high-pressure precision balance system and the reaction furnace system, fastening the annular coupling piece, and placing the sample loader in a constant-temperature section of the high-pressure reaction tube; opening an air source, and adjusting an air source pressure adjusting valve; setting the reaction gas (H)2、CO2、N2) Protective gas (N)2) Furnace gas (N)2) And a gas (N) for charging2) After the pressure of the system is reached, the flow of the pressurizing gas is set to be zero, and the experimental pressure is adjusted through a high-pressure precise control valve; starting a high-pressure gas preheater and a reactor outlet for heat tracing, setting a programmed heating method, starting a reaction at a heating rate of 10-150 ℃/min to 800 ℃, recording and analyzing weightlessness data of a high-pressure balance and data of each temperature and pressure measuring point, and introducing gas generated by the reaction into an online gas chromatography detector through a connecting pipeline for separation and analysis; and after the experiment is finished, setting the flow of the reaction gas to be zero, closing the gas preheater, the reactor outlet heat tracing element and the electric heating element, and reducing the pressure to normal pressure through a high-pressure regulating valve according to the pressure relief rate of 100KPa/min to reduce the temperature. Waiting for temperatureThe temperature is reduced to below 150 ℃, and the flow of protective gas and furnace gas is set to be zero; and taking down the sealing ring coupling piece, lifting the high-pressure precision balance system to a certain height, taking down the sample loader, collecting residual substances in the sample loader, and weighing and recording.
From the figures 2-1 to 2-4, the device can complete condition tests of different pressure grades, different heating rates, various atmospheres and different raw materials, and the test data has strong regularity and repeatability.
From the figures 2-5, the device can be used for obtaining full-component oil samples under different conditions and carrying out qualitative analysis by combining GC-MS.
Example 2
Switching on a power supply, lifting the high-pressure precision balance system to a certain height, putting a certain amount of raw materials into a sample loader, closing the high-pressure precision balance system and the reaction furnace system, fastening the annular coupling piece, and loading the sample into a constant-temperature section of the tubular reactor on the upper part of the thermocouple; opening an air source, and adjusting an air source pressure adjusting valve to enable the air source pressure to be about 4.5MPa and the experimental pressure to be 4.0 MPa; setting the reaction gas (N)2/CO2) Protective gas (N)2) Furnace gas (N)2) And a gas (N) for charging2) After the pressure of the system is reached, the flow of the pressurizing gas is set to be zero, and the experimental pressure is adjusted through a high-pressure precise control valve; starting a high-pressure gas preheater and a reactor outlet for heat tracing, setting a programmed heating method, starting reaction at a temperature rising rate of 30 ℃/min to 1000 ℃, keeping the temperature for 1h, recording and analyzing weightlessness data of a high-pressure balance and data of various temperature and pressure measuring points, introducing gas generated by the reaction into an online gas chromatography detector through a connecting pipeline for separation and analysis, and switching the reaction gas into CO when the temperature reaches 500 DEG C2. And after the experiment is finished, setting the flow of the reaction gas to be zero, closing the gas preheater, the reactor outlet heat tracing element and the electric heating element, and reducing the pressure to normal pressure through a high-pressure regulating valve according to the pressure relief rate of 100KPa/min to reduce the temperature. When the temperature is reduced to below 150 ℃, the flow of the protective gas and the flow of the furnace gas are set to be zero; taking off the sealing ring coupling piece, lifting the high-pressure precision balance system to a certain height, taking off the sample loader, collecting residual substances in the sample loader, and weighing and recording. It can be seen from fig. 3 that the apparatus can perform a high pressure gasification test to evaluate the gasification reaction activity of the feedstock.
Example 3
Switching on a power supply, lifting a high-pressure precision balance system to a certain height, putting a certain amount of raw materials (coal and catalyst) into a sample loader, closing the high-pressure precision balance system and a reaction furnace system, fastening an annular coupling piece, and placing the sample loader in a constant-temperature section of a high-pressure reaction tube; opening an air source, and adjusting an air source pressure adjusting valve to enable the air source pressure to be about 4.5MPa and the experimental pressure to be 4.0 MPa; setting the reaction gas (H)2/CO2/N22/2/1 mixed gas), shielding gas (N)2) Furnace gas (N)2) And a gas (N) for charging2) After the pressure of the system is reached, the flow of the pressurizing gas is set to be zero, and the experimental pressure is adjusted through a high-pressure precise control valve; starting a high-pressure gas preheater and a reactor outlet for heat tracing, setting a programmed heating method, starting the reaction at the heating rate of 10 ℃/min to 900 ℃, recording and analyzing the weight loss data of the high-pressure balance and the data of each temperature and pressure measuring point, and introducing the gas generated by the reaction into an online gas chromatography detector through a connecting pipeline for separation and analysis. And after the experiment is finished, setting the flow of the reaction gas to be zero, closing the gas preheater, the reactor outlet heat tracing element and the electric heating element, and reducing the pressure to normal pressure through a high-pressure regulating valve according to the pressure relief rate of 100KPa/min to reduce the temperature. When the temperature is reduced to below 150 ℃, the flow of the protective gas and the flow of the furnace gas are set to be zero; and taking down the sealing ring coupling piece, lifting the high-pressure precision balance system to a certain height, taking down the sample loader, collecting residual substances in the sample loader, and weighing and recording. As can be seen from FIG. 4, the device can complete the catalytic pyrolysis experiment and evaluate the performance of the catalyst.
Claims (7)
1. A multi-functional high pressure reaction evaluation device which characterized in that: including high-pressure precision balance system, reaction furnace system, oil gas cooling recovery system, gaseous online sampling and gas circuit control system:
the high-pressure precision balance system comprises a protective shell (2) which is fixedly arranged on one side of a lifting system (4) and is provided with a protective gas inlet (3), a high-pressure hanging arm type precision balance (1) is sealed in the protective shell (2), the lower end of the high-pressure hanging arm type precision balance (1) is connected with one end of a sample lifting hook (8), and the other end of the sample lifting hook (8) is connected with a sample loader (9);
the reaction furnace system comprises a high-pressure furnace body (5) with a furnace gas inlet (10) and a furnace gas outlet (11), and an electric heating element (6) and a high-pressure reaction tube (7) which are arranged in the high-pressure furnace body (5), the high-pressure reaction tube (7) is provided with a high-pressure furnace body (5) extending out of two ends, the upper end of the high-pressure reaction tube (7) is coupled with a high-pressure precision balance system, a sample lifting hook (8) and a sample loader (9) are vertically arranged in the high-pressure reaction tube (7), the wall of the high-pressure reaction tube (7) extending out of the upper end of the high-pressure furnace body (5) is provided with a heat tracing device (22) connected with an oil-gas cooling and recycling system, the wall of the high-pressure reaction tube (7) extending out of the lower end of the high-pressure furnace body (5) is provided with a reaction gas inlet (12) and a multielement thermocouple interface (13) from top to bottom, and a temperature measuring element is arranged in the high-pressure reaction tube (7) and is connected with the multielement thermocouple interface (13);
the oil gas cooling recovery system comprises a primary cooling section (23), a secondary cooling section (24), a high-pressure filter element (25), a high-pressure precise control valve (26) and a ball valve (27), which are sequentially connected in the flowing direction, wherein a charging gas inlet (29) is arranged between the high-pressure precise control valve (26) and the high-pressure filter element (25), an online gas chromatography detector (28) is also connected between the high-pressure precise control valve (26) and the ball valve (27), and the primary cooling section (23) is connected with a heat tracing device (22);
the gas path control system comprises a gas source pressure regulating valve (17), a gas flow controller (16), a high-pressure gas hedging mixer (15) and a high-pressure gas preheater (14) which are sequentially connected in a tap flow direction, wherein the high-pressure gas preheater (14) is communicated with a reaction gas inlet (12), one path of a gas source, which is used as a reaction gas, enters the high-pressure gas hedging mixer (15) through the gas source pressure regulating valve (17) and the gas flow controller (16) enters from the reaction gas inlet (12) through the high-pressure gas preheater (14), and the other three paths of the gas source are respectively connected with a protective gas inlet (3), a furnace gas inlet (10) and a charging gas inlet (29);
the precision of the high-pressure cantilever type precision balance (1) is 1 mu g, the sample loading amount of the sample loader (9) is 2-10 g, the highest reaction temperature of the high-pressure reaction tube (7) is 1300 ℃, the reaction pressure is 0.001-7.0 MPa, and the heating rate is 50-150 ℃/min;
the primary cooling section (23) is a natural convection cooling section, the secondary cooling section (24) is a forced convection cooling section, the two sections of pipelines are connected by high-pressure detachable clamping sleeves, and cooled gas passes through a high-pressure filter element (25) and then is subjected to gas online sampling and online gas chromatography analysis;
the temperature from the outlet of the high-pressure reaction tube (7) to the primary cooling section (23) is 350-500 ℃, one or more combinations of oleophylic adsorptive material quartz cotton, porous carbon material and oleophylic fiber material are filled in the primary cooling section (23), the temperature of the secondary cooling section (24) is-20-0 ℃, a solvent method is adopted to wash and collect a cooling oil sample, namely one or more combinations of volatile solvents of dichloromethane, petroleum ether, acetone and diesel oil are adopted to wash a pipeline of the secondary cooling section (24), and the cooling oil sample is collected.
2. The multifunctional high-pressure reaction evaluation device according to claim 1, characterized in that: the high-pressure precision balance system is connected with the inner coupling surface of the high-pressure reaction tube in a mode of combining a high-pressure sealing ring (21) with an annular coupling piece (22).
3. The multifunctional high-pressure reaction evaluation device according to claim 1, characterized in that: the heat tracing device (22) adopts one or more combinations of electric heat tracing, steam heat tracing or oil bath heat tracing.
4. The multifunctional high-pressure reaction evaluation device according to claim 1, characterized in that: the high-pressure filter element (25) is one or a combination of a metal sintering device and a ceramic filter screen, the particle size of the trapped particles is less than 200 mu m, and the high-pressure precision control valve (26) is a pneumatic regulating valve.
5. The multifunctional high-pressure reaction evaluation device according to claim 1, characterized in that: the gas source adopts a reactionThe gas is one or more of nitrogen, hydrogen, carbon dioxide, carbon monoxide, air, methane and water vapor, and the reaction includes thermal cracking reaction, catalytic reaction, pyrolysis reaction, gasification reaction, and CO2And (4) performing active reaction.
6. The multifunctional high-pressure reaction evaluation device according to claim 1, characterized in that: the high-pressure gas counter-flushing mixer (15) is a multi-channel counter-flushing mixer, the temperature of the reaction gas preheated by the high-pressure gas preheater (14) is more than or equal to 300 ℃, and the inlet of the high-pressure gas counter-flushing mixer (15) is also connected with an electric heating steam generator (18) with a micro plunger pump (19).
7. A multifunctional high-pressure reaction evaluating method of the apparatus of any one of claims 1 to 5, characterized by comprising the steps of:
1) sample loading: placing the weighed sample in a sample loader (9), and closing a high-pressure precision balance system and a reaction furnace system through a lifting system (4);
2) heating for reaction: opening an air source, and adjusting an air source pressure adjusting valve (17) to enable the air source pressure to be 0.5-1.0 MPa higher than the experimental pressure; setting gas flow (16) of reaction gas, protective gas, furnace gas and pressurized gas, setting the pressurized gas flow to be zero after the system pressure is reached, and controlling the experimental pressure through a high-pressure regulating valve (26); starting a high-pressure gas preheater (14), a reactor outlet heat tracing device (22) and an electric heating element (6), starting reaction when the temperature meets the experimental requirements, and recording and analyzing weightlessness data of a high-pressure balance and data of each temperature and pressure measuring point; simultaneously, gas generated by the reaction is introduced into an online gas chromatography detector (28) through a connecting pipeline for separation and analysis;
3) cooling the reactor: after the experiment is finished, setting the flow of the reaction gas to be zero, closing the high-pressure gas preheater (14), the reactor outlet heat tracing (22) and the electric heating element (6), reducing the pressure to normal pressure through a high-pressure regulating valve (26) according to the pressure relief rate required by the experiment, cooling, and setting the flow of the protective gas and the furnace gas to be zero when the temperature is reduced to 50-200 ℃; the ring coupling ring is removed, the high pressure precision balance system is lifted to remove the sample loader (9), and the residual substances are collected and weighed.
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